CN109680360A - Poly- fragrant oxadiazoles fiber of a kind of original liquid coloring and preparation method thereof - Google Patents

Poly- fragrant oxadiazoles fiber of a kind of original liquid coloring and preparation method thereof Download PDF

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Publication number
CN109680360A
CN109680360A CN201811634333.4A CN201811634333A CN109680360A CN 109680360 A CN109680360 A CN 109680360A CN 201811634333 A CN201811634333 A CN 201811634333A CN 109680360 A CN109680360 A CN 109680360A
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CN
China
Prior art keywords
poly
stoste
fiber
fragrant oxadiazoles
oxadiazoles
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Pending
Application number
CN201811634333.4A
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Chinese (zh)
Inventor
姚淑焕
吴萌
李文涛
张超波
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JIANGSU BAODE NEW MATERIAL CO Ltd
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JIANGSU BAODE NEW MATERIAL CO Ltd
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Application filed by JIANGSU BAODE NEW MATERIAL CO Ltd filed Critical JIANGSU BAODE NEW MATERIAL CO Ltd
Priority to CN201811634333.4A priority Critical patent/CN109680360A/en
Publication of CN109680360A publication Critical patent/CN109680360A/en
Pending legal-status Critical Current

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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/94Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/08Polyhydrazides; Polytriazoles; Polyaminotriazoles; Polyoxadiazoles
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/06Dyes

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Coloring (AREA)

Abstract

The invention discloses a kind of preparation methods of the poly- fragrant oxadiazoles fiber of original liquid coloring, its main feature is that carrying out in accordance with the following steps: dyestuff is added in 98% concentrated sulfuric acid, is slowly dissolved in concentrated sulfuric acid, chromogen liquid by the preparation of poly- virtue oxadiazoles stoste;Poly- fragrant oxadiazoles stoste after aromatic diacid is polymerize with hydrazonium salt is cooled to 90-100 DEG C in polymeric kettle;After poly- fragrant oxadiazoles stoste drops to 90-100 DEG C, chromogen liquid is slowly added into poly- fragrant oxadiazoles stoste, it is stirring while adding, while controlling poly- fragrant oxadiazoles stoste temperature and must not exceed 100 DEG C;It is to be mixed uniformly after, carry out deaeration into deaerator, carry out wet spinning after the completion of deaeration, coloured fiber is made, fiber color is uniform and bright-coloured.It is an advantage of the invention that original liquid coloring method is by adding colorant in fiber stoste, coloring and spinning can be carried out continuously simultaneously, uniform coloring, good color fastness, and dye-uptake is high, with short production cycle.At low cost, pollution is also few.

Description

Poly- fragrant oxadiazoles fiber of a kind of original liquid coloring and preparation method thereof
Technical field
The invention belongs to the poly- fragrant oxadiazoles fiber of macromolecular fibre technical field more particularly to a kind of original liquid coloring and its systems Preparation Method.
Background technique
Poly- virtue oxadiazoles fiber true qualities are faint yellow or yellow, and color is more single, but due to it in occupational protection and The application of apparel industry proposes the more abundant requirement of color to the color of fiber.The dyestuff for the POD dyeing reported at present Including acid dyes, the dye of positive ion, disperse dyes and reactive dye, but net assessment gets off, reactive dye K/S value compared with Low, acid dyes and dye of positive ion crock fastness are poor, and the sample light fastness of disperse dyeing is relatively low, only Disperse dyeing effect is more excellent, and disperse dyeing process temperature is high, of long duration, but unfriendly to environment.
Summary of the invention
In order to overcome the deficiencies of the prior art, the purpose of the present invention is to provide a kind of poly- fragrant oxadiazoles fiber of original liquid coloring and Preparation method, coloring and spinning are carried out continuously simultaneously, and uniform coloring, good color fastness, dye-uptake is high, with short production cycle, cost Low, pollution is also few.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of the poly- fragrant oxadiazoles fiber of original liquid coloring, its main feature is that carrying out in accordance with the following steps:
The preparation of the poly- fragrant oxadiazoles stoste of step 1;
The preparation of step 2 chromogen liquid: dyestuff is added in 98% concentrated sulfuric acid, is slowly dissolved in concentrated sulfuric acid, forms m%'s Chromogen liquid;
Poly- fragrant oxadiazoles stoste after aromatic diacid polymerize by step 3 with hydrazonium salt is cooled to 90-100 in polymeric kettle ℃;
It is former that step 4 is slowly added into poly- fragrant oxadiazoles after poly- fragrant oxadiazoles stoste drops to 90-100 DEG C, by chromogen liquid It is stirring while adding in liquid, while controlling poly- fragrant oxadiazoles stoste temperature and must not exceed 100 DEG C;
Step 5 it is to be mixed uniformly after, carry out deaeration into deaerator, carry out wet spinning after the completion of deaeration, coloring is made Fiber.
Further, gather in the step 3 and step 4 after fragrant oxadiazoles stoste drops to 90 DEG C, chromogen liquid is slowly added Enter into poly- fragrant oxadiazoles stoste.
Original liquid coloring is that colorant appropriate is added in spinning solution, can also by adequately mixing, dissolving and filtering Quantitative injection toner or coloured stoste before entering spinning head, are spun into colored fibre after static mixer mixes.It is viscous The original liquid coloring of the fibers such as glue/acrylic fibers belongs to such.This technique of original liquid coloring belongs to physical change, and advantage is coloring and spins Silk can be carried out continuously simultaneously, uniform coloring, good color fastness, and dye-uptake is high, with short production cycle, at low cost, and pollution is few.
Containing polar group as oxadiazoles ring and hydrazides group in POD molecule, it is good to guarantee that fiber and dyestuff have Affinity interaction power so that dyeing is carried out, as observation using wet spinning made from the fibre section POD and surface The scanning electron microscope (SEM) photograph of form does not have the defects of hole it can be seen that fibre structure is finer and close, but cross sectional shape is irregular, has Skin-core structure, fiber surface have obvious longitudinal groove structure, and rough surface is conducive to dyestuff and enters fibrous inside, in addition, passing through XRD detection shows that the crystallinity of fiber is not high, and the stainability of fiber is also relatively good.
A kind of poly- fragrant oxadiazoles fiber of original liquid coloring, its main feature is that the poly- fragrant oxadiazoles fiber of the original liquid coloring is by above-mentioned system Preparation Method is prepared.
Compared with prior art, it is an advantage of the invention that original liquid coloring method be by adding colorant in fiber stoste, Coloring and spinning can be carried out continuously simultaneously, uniform coloring, good color fastness, and dye-uptake is high, with short production cycle.It is at low cost, pollution It is few.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
A kind of preparation method of the poly- fragrant oxadiazoles fiber of original liquid coloring, its main feature is that carrying out in accordance with the following steps:
The preparation of the poly- fragrant oxadiazoles stoste of step 1;
The preparation of step 2 chromogen liquid: dyestuff being added in 98% concentrated sulfuric acid, be slowly dissolved in concentrated sulfuric acid, forms chromogen Liquid;
Poly- fragrant oxadiazoles stoste after aromatic diacid polymerize by step 3 with hydrazonium salt is cooled to 90 DEG C in polymeric kettle;
Chromogen liquid is slowly added into poly- fragrant oxadiazoles stoste by step 4 after poly- fragrant oxadiazoles stoste drops to 90 DEG C, It is stirring while adding, while controlling poly- fragrant oxadiazoles stoste temperature and must not exceed 100 DEG C;
Step 5 it is to be mixed uniformly after, carry out deaeration into deaerator, carry out wet spinning after the completion of deaeration, coloring is made Fiber, fiber color are uniform and bright-coloured.

Claims (3)

1. a kind of preparation method of the poly- fragrant oxadiazoles fiber of original liquid coloring, its main feature is that carrying out in accordance with the following steps:
The preparation of the poly- fragrant oxadiazoles stoste of step 1;
The preparation of step 2 chromogen liquid: dyestuff being added in 98% concentrated sulfuric acid, be slowly dissolved in concentrated sulfuric acid, forms chromogen liquid;
Poly- fragrant oxadiazoles stoste after aromatic diacid polymerize by step 3 with hydrazonium salt is cooled to 90-100 DEG C in polymeric kettle;
Chromogen liquid is slowly added into poly- fragrant oxadiazoles stoste by step 4 after poly- fragrant oxadiazoles stoste drops to 90-100 DEG C, It is stirring while adding, while controlling poly- fragrant oxadiazoles stoste temperature and must not exceed 100 DEG C;
Step 5 it is to be mixed uniformly after, carry out deaeration into deaerator, carry out wet spinning after the completion of deaeration, coloured fiber is made.
2. the preparation method of the poly- fragrant oxadiazoles fiber of a kind of original liquid coloring according to claim 1, it is characterised in that: the step Rapid 3 and step 4 in gather after fragrant oxadiazoles stoste drops to 90 DEG C, chromogen liquid is slowly added into poly- fragrant oxadiazoles stoste.
3. a kind of poly- fragrant oxadiazoles fiber of original liquid coloring, it is characterised in that: the poly- fragrant oxadiazoles fiber of the original liquid coloring is by such as weighing Benefit requires the described in any item preparation methods of 1-8 to be prepared.
CN201811634333.4A 2018-12-29 2018-12-29 Poly- fragrant oxadiazoles fiber of a kind of original liquid coloring and preparation method thereof Pending CN109680360A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811634333.4A CN109680360A (en) 2018-12-29 2018-12-29 Poly- fragrant oxadiazoles fiber of a kind of original liquid coloring and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811634333.4A CN109680360A (en) 2018-12-29 2018-12-29 Poly- fragrant oxadiazoles fiber of a kind of original liquid coloring and preparation method thereof

Publications (1)

Publication Number Publication Date
CN109680360A true CN109680360A (en) 2019-04-26

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030129398A1 (en) * 2000-06-28 2003-07-10 General Electric Company Process to prepare polymeric fibers with improved color and appearance
CN101735455A (en) * 2008-11-14 2010-06-16 无锡华东创新材料研究院 Method for preparing special aromatic polyoxadiazole and flame-retardant high-temperature resistant polyoxadiazole fiber thereof
CN101906674A (en) * 2010-06-30 2010-12-08 江苏宝德新材料有限公司 Efficient washing process for aromatic poly 1,3,4-oxadiazole acid-containing wet silk ribbon
CN104831400A (en) * 2015-05-22 2015-08-12 江苏宝德新材料有限公司 Low-viscosity aromatic polyoxdiazole solution and fiber prepared from same
CN107761184A (en) * 2017-10-24 2018-03-06 四川大学 A kind of original liquid coloring composite fibre and preparation method thereof
CN108385193A (en) * 2018-03-06 2018-08-10 天津工业大学 A kind of preparation method of the coloured nanofiber of polyamide 6/tetracarboxylic acid dianhydride

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030129398A1 (en) * 2000-06-28 2003-07-10 General Electric Company Process to prepare polymeric fibers with improved color and appearance
CN101735455A (en) * 2008-11-14 2010-06-16 无锡华东创新材料研究院 Method for preparing special aromatic polyoxadiazole and flame-retardant high-temperature resistant polyoxadiazole fiber thereof
CN101906674A (en) * 2010-06-30 2010-12-08 江苏宝德新材料有限公司 Efficient washing process for aromatic poly 1,3,4-oxadiazole acid-containing wet silk ribbon
CN104831400A (en) * 2015-05-22 2015-08-12 江苏宝德新材料有限公司 Low-viscosity aromatic polyoxdiazole solution and fiber prepared from same
CN107761184A (en) * 2017-10-24 2018-03-06 四川大学 A kind of original liquid coloring composite fibre and preparation method thereof
CN108385193A (en) * 2018-03-06 2018-08-10 天津工业大学 A kind of preparation method of the coloured nanofiber of polyamide 6/tetracarboxylic acid dianhydride

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Application publication date: 20190426

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